CN208839602U - Double stationary phase gas chromatographic columns - Google Patents
Double stationary phase gas chromatographic columns Download PDFInfo
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- CN208839602U CN208839602U CN201820970265.8U CN201820970265U CN208839602U CN 208839602 U CN208839602 U CN 208839602U CN 201820970265 U CN201820970265 U CN 201820970265U CN 208839602 U CN208839602 U CN 208839602U
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Abstract
The utility model provides a kind of double stationary phase gas chromatographic columns, comprising: substrate is formed with micro- channel in substrate, and micro- channel has first port and second port；Encapsulation cover plate, is bonded to substrate surface, and encapsulation cover plate closes the microchannel of micro- channel shape stationary phase gas chromatographic column in pairs；And first stationary phase and the second stationary phase, it is formed in the inner surface of the bottom of micro- channel, side wall and the corresponding encapsulation cover plate being located above micro- channel, and the first stationary phase, close to first port, the second stationary phase is close to second port.Double stationary phase gas chromatographic columns provided by the utility model and preparation method thereof, the coating of two kinds of stationary phases is realized on same gas chromatographic column, a gas chromatographic column is enabled to separate two class mixing gas components well, enhance the separating capacity of gas chromatographic column, reduce the frequency for replacing gas chromatographic column when identifying variety classes mixing gas component in order to separate simultaneously, uses more convenient.
Description
Technical field
The utility model belongs to microelectromechanical systems field, more particularly to a kind of double stationary phase gas chromatographic columns.
Background technique
The major function of gas chromatographic column is separated to mixing sample gas to be analyzed, it is gas chromatograph
Core component.Traditional gas chromatographic column includes capillary column, packed column etc..From chromatographic column prepare material from the point of view of, it is traditional
Gas chromatographic column generally uses glass, stainless steel processing and fabricating, is widely used at present.And since 1970s,
People begin trying to make micro-scale gas chromatograph column by corrosion/etching method on silicon wafer or sheet glass.
The separation function of gas chromatographic column is by the interaction between mixing sample gas to be analyzed and stationary phase
It realizes.Currently, using, research gas chromatographic column inside be only prepared with a kind of stationary phase, this stationary phase is usually single
Substance, it is however generally that, certain class gas component can only be separated, and when another kind of gas component to be separated, then it needs replacing
Gas chromatographic column, it is inconvenient to use.
Therefore, how a kind of double stationary phase gas chromatographic columns are provided, it is real to solve above-mentioned technical problem in the prior art
Belong to necessary.
Utility model content
In view of the foregoing deficiencies of prior art, the purpose of this utility model is to provide a kind of double stationary phase gas phase colors
Column is composed, for solving the problems such as gas chromatographic column can only be separated to certain class gas component, is inconvenient to use in the prior art.
In order to achieve the above objects and other related objects, the utility model provides a kind of system of double stationary phase gas chromatographic columns
Preparation Method includes the following steps:
1) substrate is provided, micro- channel is made in Yu Suoshu substrate, micro- channel has first port and second port；
2) configured first stationary phase raw material is injected from the first port, and injects the first stationary phase raw material
To a predeterminated position of micro- channel；
3) structure for obtaining step 2) is placed in vacuum cavity, is fixed so that the first stationary phase raw material forms first
Phase；
4) structure that step 3) obtains is taken out, configured second stationary phase raw material is injected from the second port, and
Inject the predeterminated position of the second stationary phase raw material to micro- channel；And
5) structure for obtaining step 4) is placed in vacuum cavity, is fixed so that the second stationary phase raw material forms second
Phase.
As a kind of preferred embodiment of the utility model, in step 2), the first stationary phase raw material is injected to described pre-
If sealing the second port behind position, and the second port is opened after step 4) takes out the structure that step 3) obtains；Step
It is rapid 4) in, seal the first port after injecting the second stationary phase raw material to the predeterminated position, and after step 5)
Open the first port.
As a kind of preferred embodiment of the utility model, the first port and the second port are realized using sealant
Sealing, and open the first port and the second port by way of removing the sealant.
As a kind of preferred embodiment of the utility model, in step 2), the first stationary phase raw material includes poly dimethyl
Any one in siloxane solution and polymethylphenylsiloxane solution, in step 4), the second stationary phase raw material includes
Any one in dimethyl silicone polymer solution and polymethylphenylsiloxane solution, and the first stationary phase raw material and institute
It is different to state the second stationary phase raw material.
As a kind of preferred embodiment of the utility model, the temperature in vacuum cavity in step 3) is between 24 DEG C -150 DEG C
Between, by structure that step 2) obtains in the time placed in vacuum cavity between -72h for 24 hours；Vacuum chamber in step 5)
Temperature in body between 24 DEG C -150 DEG C, the time that the structure that step 4) is obtained is placed in vacuum cavity between for 24 hours -
Between 72h.
As a kind of preferred embodiment of the utility model, step 1) further includes providing an encapsulation cover plate, by the cap
Plate is bonded with the substrate, to close the microchannel that micro- channel forms double stationary phase gas chromatographic columns.
As a kind of preferred embodiment of the utility model, the encapsulation cover plate includes the glass cover-plate of twin polishing, is used
The encapsulation cover plate is bonded by anode linkage method with the substrate.
As a kind of preferred embodiment of the utility model, perspective view of the micro- channel in the plane where the substrate
The serpentine-like shape of shape, and the edge of the projecting figure is in broken line shape.
As a kind of preferred embodiment of the utility model, first stationary phase edge corresponds to the shape of the projecting figure
It is different from the shape of the corresponding projecting figure in second stationary phase edge.
As a kind of preferred embodiment of the utility model, also with the micro-structure list of multiple array arrangements in micro- channel
Member.
As a kind of preferred embodiment of the utility model, the bottom of micro- channel, side wall and the microstructure unit
Silicon nanowires forest structure is formed at least one of surface.
The utility model also provides a kind of double stationary phase gas chromatographic columns, comprising:
Substrate is formed with micro- channel in the substrate, and micro- channel has first port and second port；
Encapsulation cover plate, is bonded to the substrate surface, and the encapsulation cover plate closing micro- channel forms described double fixed
The microchannel of phase gas chromatographic column；And
First stationary phase and the second stationary phase, bottom, side wall and the correspondence for being formed in micro- channel are located at micro- ditch
The inner surface of the encapsulation cover plate above road, and first stationary phase is close to the first port, second stationary phase
Close to the second port.
As a kind of preferred embodiment of the utility model, side and institute of first stationary phase far from the first port
The second stationary phase is stated to be in contact far from the side of the second port.
As a kind of preferred embodiment of the utility model, first stationary phase includes dimethyl silicone polymer layer and poly- first
Any one in base phenyl siloxane layer, second stationary phase includes dimethyl silicone polymer layer and polymethyl-benzene base silicon oxygen
Any one in alkane layer, first stationary phase is different from second stationary phase.
As a kind of preferred embodiment of the utility model, perspective view of the micro- channel in the plane where the substrate
The serpentine-like shape of shape, and the edge of the projecting figure is in broken line shape.
As a kind of preferred embodiment of the utility model, first stationary phase edge corresponds to the shape of the projecting figure
It is different from the shape of the corresponding projecting figure in second stationary phase edge.
As a kind of preferred embodiment of the utility model, also with the micro-structure list of multiple array arrangements in micro- channel
Member.
As a kind of preferred embodiment of the utility model, the bottom of micro- channel, side wall and the microstructure unit
Silicon nanowires forest structure is formed at least one of surface.
As described above, double stationary phase gas chromatographic columns of the utility model, have the advantages that the utility model mentions
The double stationary phase gas chromatographic columns supplied, realize two kinds of stationary phases by simple and convenient method on same gas chromatographic column
Coating, enables a gas chromatographic column to separate two class mixing gas components well, enhances the separation energy of gas chromatographic column
Power, while reducing the frequency that gas chromatographic column is replaced when identifying variety classes mixing gas component in order to separate, it uses
It is more convenient.Meanwhile being optimized by micro- channel shape to different fixed opposite positions, to be advantageously implemented same type
The separation of mixing gas component.
Detailed description of the invention
Fig. 1 is shown as the preparation technology flow chart of double stationary phase gas chromatographic columns provided by the utility model.
Fig. 2 is shown as providing the knot for being formed with micro- channeled substrate in double stationary phase gas chromatographic columns preparation of the utility model
Structure schematic diagram.
Fig. 3 is shown as the top view of the micro- channel formed in double stationary phase gas chromatographic columns preparation of the utility model.
Fig. 4 is shown as forming the first stationary phase and the second fixation in double stationary phase gas chromatographic columns preparation of the utility model
Phase schematic diagram.
Fig. 5 is shown as forming the first stationary phase and the second fixation in double stationary phase gas chromatographic columns preparation of the utility model
Phase perspective view.
Fig. 6 is shown as being formed with double stationary phase gas chromatographic columns signal of microtrabeculae in micro- channel provided by the utility model
Figure.
Component label instructions
100 substrates
101 micro- channels
The bottom 101a
101b side wall
102 first ports
103 second ports
104 predeterminated positions
105 first stationary phases
106 second stationary phases
107 microstructure units
S1~S5 step 1) is to step 5)
Specific embodiment
Illustrate the embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this theory
Content disclosed by bright book understands other advantages and effect of the utility model easily.The utility model can also be by addition
Different specific embodiments are embodied or practiced, and the various details in this specification can also be based on different viewpoints and answer
With carrying out various modifications or alterations under the spirit without departing from the utility model.
Fig. 1 is please referred to Fig. 6.It should be noted that diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of utility model, though it is only shown with related component in the utility model rather than when according to actual implementation in diagram
Component count, shape and size are drawn, when actual implementation form, quantity and the ratio of each component can arbitrarily change for one kind
Become, and its assembly layout form may also be increasingly complex.
As shown in Figure 1, the utility model provides a kind of preparation method of double stationary phase gas chromatographic columns, including walk as follows
It is rapid:
1) substrate is provided, micro- channel is made in Yu Suoshu substrate, micro- channel has first port and second port；
2) configured first stationary phase raw material is injected from the first port, and injects the first stationary phase raw material
To a predeterminated position of micro- channel；
3) structure for obtaining step 2) is placed in vacuum cavity, is fixed so that the first stationary phase raw material forms first
Phase；
4) structure that step 3) obtains is taken out, configured second stationary phase raw material is injected from the second port, and
Inject the predeterminated position of the second stationary phase raw material to micro- channel；And
5) structure for obtaining step 4) is placed in vacuum cavity, is fixed so that the second stationary phase raw material forms second
Phase.
The preparation process of double stationary phase gas chromatographic columns of the utility model is described in detail below in conjunction with attached drawing.
Firstly, carrying out step 1) shown in S1 and Fig. 2 and Fig. 3 as shown in figure 1, providing a substrate 100, Yu Suoshu substrate
Micro- channel 101 is made in 100, micro- channel has first port 102 and second port 103.
As an example, projecting figure serpentine-like shape of the micro- channel 101 in the plane where the substrate 100.
As an example, the edge of the projecting figure is in broken line shape.
As an example, 105 edge of the first stationary phase corresponds to the shape and second stationary phase of the projecting figure
The shape that 106 edges correspond to the projecting figure is different.
Specifically, providing a substrate 100 first, it is used to form the microchannel of subsequent production gas chromatographic column, the substrate
100 can choose as silicon substrate, but be not limited thereto.In addition, micro- channel 101 is made in the substrate 100, it is described micro-
Channel 101 includes bottom 101a and side wall 101b, and micro- channel 101 can be prepared using photoetching-etching technique, described
Grown silicon nitride film on substrate 100, and spin coating photoresist form covering for silicon nitride and photoresist using photo etching process
Then mould figure makes micro- channel 101 using DRIE technique in the substrate 100.Wherein, in a preferred embodiment, institute
Stating micro- channel 101 can extend in round-trip bending, and such as serpentine-like shape, bending angle and length etc. are selected according to actual demand.
In addition, the first port 102 and the second port 103 are preferably provided at micro- channel for making micro-fluidic port
101 both ends.
In addition, in a preferred embodiment, the side wall of the edge of the projecting figure namely micro- channel 101
Pattern includes broken line shape, such as irregular fold-line-shaped, rule or irregular waveform, square waveform and triangular waveform,
Rule or irregular zigzag etc., can be using the techniques preparation such as etching well known in the art, the side wall of micro- channel 101
Above-mentioned pattern setting, be conducive to the control of flow rate of carrier gas, be further conducive to carrier gas between two stationary phases of the application
Distribution, further, it is possible to different shapes is arranged on the side wall of the different corresponding micro- channels of fixation, such as corresponding first
The side wall of micro- channel 101 of 105 position of stationary phase is serrated, the side wall of micro- channel 101 of corresponding second stationary phase, 106 position
Wavy shape, so as to realize effective cooperation that different stationary phases are carried out in gas centrifugation.
Then, shown in S2 as shown in figure 1, step 2) is carried out, by configured first stationary phase raw material (solution or suspension
Or emulsion) injected from the first port 102, and the first stationary phase raw material is injected to a default position of micro- channel
Set 104.
Continue, shown in S3 as shown in figure 1 and Fig. 4~6, carries out step 3), the structure that step 2) is obtained is placed in vacuum chamber
In body, so that the first stationary phase raw material forms the first stationary phase 105.
As an example, in step 2), injects after the first stationary phase raw material to the predeterminated position 104 and seal described the
Two-port netwerk 103.As an example, sealing the second port 103 using sealant.
Specifically, preparing the first stationary phase 105 in the structure of step 1), the first stationary phase raw material is used to form
One stationary phase, wherein the first stationary phase raw material can be the flow-like that is in a liquid state, and can be solution or suspension or milkiness
The configured first stationary phase raw material is pushed by liquid from the first port 102 first, until a predeterminated position 104, stops
Thrust enters the first stationary phase raw material, wherein in a preferred embodiment, by coating sealant in second port 103
The second port 103 is sealed, certainly, the natural flow effect of the first stationary phase raw material can be ignored after sealing, at this point,
The structure being sealed is placed in a vacuum cavity, and is stood, during standing, the solvent in the first stationary phase raw material is gradually
The preparation of the first stationary phase 105 is completed in volatilization.
Specifically, position, the size of the predeterminated position 104 according to the first stationary phase actually required etc. determines, in addition,
The first stationary phase raw material includes in dimethyl silicone polymer (PDMS) solution and polymethylphenylsiloxane (PMPS) solution
Any one, dimethyl silicone polymer is low pole stationary phase, suitable for analyze the compound of nonpolarity or low pole, as just
Structure alkane etc.；And polymethylphenylsiloxane is especially suitable for analyzing aromatic compounds, in a preferred embodiment, Ke Yixuan
Select the PDMS solution for being 4% as solvent dose volume percent concentration using pentane；Alternatively, selecting to prepare body by solvent of toluene
The PMPS solution that product percent concentration is 1.7%, in addition, the concentration of the first stationary phase raw material can select as needed,
Above-mentioned concentration is not limited to, in a preferred embodiment, the thickness of finally formed first stationary phase 105 is according to described in
The concentration decision of first stationary phase raw material, thickness of the concentration of the first stationary phase raw material according to the first stationary phase 105 needed
Degree selection, certainly, in other examples, the first stationary phase raw material can also be other gas chromatographic column stationary phases that can be used as
Solution, according to actual selection.
As an example, the temperature in vacuum cavity in step 3) obtains between 24 DEG C -150 DEG C, and by step 2)
Structure in the time placed in vacuum cavity between -72h for 24 hours.
Specifically, rate-determining steps 2) temperature and time placed in a vacuum of obtained structure, it is solid to obtain excellent two
Determine the performance of phase, the knot that the temperature in vacuum cavity in step 3) is preferably between 30 DEG C -60 DEG C, and step 2) is obtained
Structure is preferably between 45h-50h in the time placed in vacuum cavity, in addition, herein " between ... between " refer to wrapping
The numberical range of the point value containing both ends.
Then, shown in S4 as shown in figure 1, step 4) is carried out, the structure that step 3) obtains is taken out, configured second is consolidated
Determine phase raw material (solution or suspension or emulsion) to inject from the second port 103, and injects the second stationary phase raw material
To the predeterminated position 104 of micro- channel 101；
Finally, carrying out step 5) shown in S5 as shown in figure 1 and Fig. 4~6, the structure that step 4) is obtained is placed in vacuum chamber
In body, so that the second stationary phase raw material forms the second stationary phase 106.
As an example, opening the second port 103 after step 4) takes out the structure that step 3) obtains；And step 4)
In, inject after the second stationary phase raw material to the predeterminated position 104 and seal the first port 102, and step 5) it
After open the first port 102.
As an example, sealing the first port 102 using sealant, and opened by way of removing the sealant
The first port 102.
Specifically, preparing the second stationary phase 106 after preparing first stationary phase 105, second stationary phase is former
Material is used to form the second stationary phase, wherein the second stationary phase raw material can be the flow-like that is in a liquid state, and can be solution or outstanding
Turbid or emulsion will form the structure after the first stationary phase 105 first and takes out from vacuum cavity, described the is removed after taking-up
Sealant on Two-port netwerk 103, then the configured second stationary phase raw material is pushed into from the second port 103, until
The predeterminated position 104 finally makes second stationary phase 106 be connected with first stationary phase 105, stops push-in institute
State the second stationary phase raw material, wherein in a preferred embodiment, by coating described in sealant sealing in first port 102
First port 102, certainly, the natural flow effect of the second stationary phase raw material can be ignored after sealing, at this point, will be sealed
Structure be placed in a vacuum cavity, and stand, during standing, the solvent in the second stationary phase raw material gradually volatilizees, complete
At the preparation of the second stationary phase 106.Specifically, first stationary phase 105 is with second stationary phase 106 in micro- channel
Arrangement length in 101 etc. is configured according to actual demand.
As an example, the second stationary phase raw material includes dimethyl silicone polymer solution and polymethyl-benzene in step 4)
Any one in radical siloxane solution, and the first stationary phase raw material is different from the second stationary phase raw material.
As an example, the temperature in vacuum cavity in step 5) obtains between 24 DEG C -150 DEG C, and by step 4)
Structure in the time placed in vacuum cavity between -72h for 24 hours.
Specifically, the second stationary phase raw material includes dimethyl silicone polymer (PDMS) solution and polymethyl-benzene base silicon oxygen
Any one in alkane (PMPS) solution, dimethyl silicone polymer are low pole stationary phase, are suitable for analysis nonpolarity or weak pole
The compound of property, such as n-alkane；And polymethylphenylsiloxane is especially suitable for analyzing aromatic compounds, it is preferable one
In embodiment, the PDMS solution for being 4% as solvent dose volume percent concentration using pentane can choose；Alternatively, selection with
Toluene is the PMPS solution that solvent dose volume percent concentration is 1.7%, in addition, the concentration of the second stationary phase raw material can
It selects as needed, does not limit to above-mentioned concentration, in a preferred embodiment, finally formed second stationary phase
106 thickness determines that the concentration of the second stationary phase raw material is according to needs according to the concentration of the second stationary phase raw material
The thickness of second stationary phase 106 selects, and certainly, in other examples, the second stationary phase raw material can also be that other can be used as
The solution of gas chromatographic column stationary phase, according to actual selection.
Specifically, rate-determining steps 4) temperature and time placed in a vacuum of obtained structure, it is solid to obtain excellent two
Determine the performance of phase, the knot that the temperature in vacuum cavity in step 5) is preferably between 30 DEG C -60 DEG C, and step 2) is obtained
Structure is preferably between 45h-50h in the time placed in vacuum cavity.
As an example, step 1) further includes, an encapsulation cover plate is provided, the encapsulation cover plate and the substrate 100 are carried out
Bonding forms the microchannel of double stationary phase gas chromatographic columns to close micro- channel 101.
As an example, the encapsulation cover plate includes the glass cover-plate of twin polishing, using anode linkage method by the envelope
Capping plate is bonded with the substrate.Bonding temperature is bonded voltage between 600-1400V between 200-450 DEG C.
As an example, the first stationary phase 105 and the second stationary phase 106, are formed in bottom, the side wall of micro- channel 101
And the inner surface of the corresponding encapsulation cover plate being located above micro- channel.
Specifically, further include the steps that preparing encapsulation cover plate during preparing double stationary phase gas chromatographic columns,
In, it closes micro- channel 101 and does not mean that completely enclosed, guarantee the microchannel for forming gas chromatographic column, the common skill in this field
Art personnel are preferably between 250-350 DEG C according to actual selection, bonding temperature, bonding voltage be preferably between 800-1000V it
Between.In a preferred embodiment, in the formation of first stationary phase and second stationary phase, first stationary phase
105 are located at the bottom and side wall of a part of micro- channel, it is preferable that first stationary phase is also corresponding to be located at micro- ditch
The inner surface of the encapsulation cover plate above road；Second stationary phase 106 be located at a part of micro- channel bottom and
Side wall, it is preferable that the inner surface of the also corresponding encapsulation cover plate being located above micro- channel of second stationary phase.
As an example, also with the microstructure unit 107 of multiple array arrangements in micro- channel 101, as shown in Figure 6.
As an example, at least one in the surface of the bottom of micro- channel 101, side wall and the microstructure unit 107
Silicon nanowires forest structure is formed on person.
Specifically, the microstructure unit 107 is set on the bottom of micro- channel 101, it is located at micro- channel 101
In the groove profile space of formation, it is preferable that the height of the microstructure unit 107 is identical as the depth of micro- channel 101,
In one preferred embodiment, micro- channel 101 extends in round-trip bending, including several end to end straight line portions and bending
Portion, wherein the microstructure unit 107 can be strip or square block, when being selected as strip, the microstructure unit
107 length is identical as the length of the straight line portion, certainly can be according to other length of actual selection, in addition, the micro-structure list
Member 107 can also be that micro- column structure, the microtrabeculae can be the micro-column structure in round or ellipse section, and size is according to practical
Demand and the selection of micro- channel width.
In addition, in a preferred embodiment, in the bottom 101a and side wall 101b of micro- channel 101, preparing micro-nano
Line forest structure, when being also formed with the microstructure unit 107 in micro- channel 101, also in the microstructure unit
The silicon nanowires forest structure is formed on surface, e.g., when being formed with micro- columnar microstructure unit in micro- channel
When, nano wire forest structure is formed at least one of micro- channel inner wall and the micro-post surface, it is preferable that
The inner wall of micro- channel 101, the surface of the microstructure unit are respectively formed on the nano wire forest structure.Wherein, described
Nano wire forest structure includes multiple silicon nanowires, and it is good that the application is prepared pattern, is evenly distributed, high density and quality is good
Good silicon nanowires forest structure, substantially increases surface area, to effectively improve the column capacity of silicon microfluidic chromatography column, separation
Degree and column effect.Preferably, the line footpath of the silicon nanowires in the silicon nanowires forest structure is between 20~80 nanometers.Specifically
, a kind of preparation process of nano wire forest structure is provided: 1) silicon substrate being put into 70ml hydrofluoric acid, 140ml deionization
10min is reacted in the mixed solution of water, to remove the oxide layer of micro- channel surface.The utility model first removes micro- ditch
To guarantee the reaction efficiency of subsequent metal Assisted Chemical Etching Process, and silicon nanowires forest knot can be improved in the oxide layer on road surface
Distributing homogeneity, density and the quality of structure；2) it the deposition of Ag: takes 1g silver nitrate to be put into 300ml aqueous solution and is configured to
The silver nitrate solution of 0.02mol/L, take 8ml concentration be 0.02mol/L silver nitrate, and with 20ml hydrofluoric acid, 60ml deionized water
It is mixed into solution, uniformly vibrates 6min for going the silicon substrate of removing oxide layer to be put into solution；3) prepared by silicon nanowires: will deposit Ag
Silicon substrate be put by 20ml hydrofluoric acid, the mixed solution that 2ml hydrogen peroxide and 30ml deionized water are prepared is heated at 40 DEG C
2.5min, heating process pay attention to uniformly vibrating；4) after corroding, silicon substrate the removal of Ag: is immersed to 68% nitric acid immediately
The silver of surface of silicon, soaking time 30min are removed in solution.
The utility model also provides a kind of double stationary phase gas chromatographic columns, wherein double stationary phase gas chromatographic columns are excellent
Choosing is prepared using the preparation method of double stationary phase gas chromatographic columns provided by the utility model, double stationary phase gas phase colors
Composing column includes:
Substrate 100, is formed with micro- channel 101 in the substrate, and micro- channel 101 has first port 102 and the
Two-port netwerk 103；
Encapsulation cover plate, is bonded to 100 surface of substrate, and the encapsulation cover plate closing micro- channel 101 forms described
The microchannel of double stationary phase gas chromatographic columns；And
First stationary phase 105 and the second stationary phase 106, bottom, side wall and the correspondence for being formed in micro- channel 101 are located at
The inner surface of the encapsulation cover plate of 101 top of micro- channel, and first stationary phase 105 is close to the first port
102, described second fixes 106 phases close to the second port 103.
Specifically, double stationary phase gas chromatographic columns provided by the utility model, realize two on same gas chromatographic column
The coating of kind of stationary phase, i.e., described first stationary phase 105 and second stationary phase 106, enable a gas chromatographic column very
Two class mixing gas components are separated well, enhance the separating capacity of gas chromatographic column, while being reduced to separate and identify not
With the frequency for replacing gas chromatographic column when type mixing gas component, use more convenient.Wherein, first stationary phase
105 are located at the bottom and side wall of a part of micro- channel, it is preferable that first stationary phase is also corresponding to be located at micro- ditch
The surface of the encapsulation cover plate above road；Second stationary phase 106 is located at the bottom and side of a part of micro- channel
Wall, it is preferable that the surface of the also corresponding encapsulation cover plate being located above micro- channel of second stationary phase.
As an example, side of first stationary phase 105 far from the first port 102 and second stationary phase
106 sides far from the second port 103 are in contact.Specifically, in this example, first stationary phase 105 and described the
It is in contact at two stationary phases, 106 phase, one predeterminated position 104, so that two fixations match, is conducive to improve gas separating capacity, institute
It states predeterminated position 104 and selects to be arranged according to actual demand.
As an example, first stationary phase 105 includes in dimethyl silicone polymer layer and polymethylphenylsiloxane layer
Any one, second stationary phase 106 includes any in dimethyl silicone polymer layer and polymethylphenylsiloxane layer
One kind, first stationary phase are different from second stationary phase.First stationary phase, second stationary phase can also be
Other can be used as gas chromatographic column stationary phase, according to actual selection.
As an example, projecting figure serpentine-like shape of the micro- channel 101 in the plane where the substrate.
As an example, the edge of the projecting figure is in broken line shape.
As an example, 105 edge of the first stationary phase corresponds to the shape and second stationary phase of the projecting figure
The shape that 106 edges correspond to the projecting figure is different.
Specifically, providing a substrate 100 first, it is used to form the microchannel of subsequent production gas chromatographic column, the substrate
100 can choose as silicon substrate, but be not limited thereto.In addition, micro- channel 101 is made in the substrate 100, it is described micro-
Channel 101 is in that round-trip bending extends, and such as serpentine-like shape, the foundation actual demand selection gist such as bending angle and length is practical to be needed
Ask selection, including bottom and side wall.The first port 102 and the second port 103 are for making micro-fluidic port, preferably
The both ends of micro- channel 101 are set.
In addition, in a preferred embodiment, the side wall of the edge of the projecting figure namely micro- channel 101
Pattern includes broken line shape, such as irregular fold-line-shaped, rule or irregular waveform, square waveform and triangular waveform,
Rule or irregular zigzag etc., can be using the techniques preparation such as etching well known in the art, the side wall of micro- channel 101
Above-mentioned pattern setting, be conducive to the control of flow rate of carrier gas, be further conducive to carrier gas between two stationary phases of the application
Distribution, further, it is possible to different shapes is arranged on the side wall of the different corresponding micro- channels of fixation, such as corresponding first
The side wall of micro- channel 101 of 105 position of stationary phase is serrated, the side wall of micro- channel 101 of corresponding second stationary phase, 106 position
Wavy shape, so as to realize effective cooperation that different stationary phases are carried out in gas centrifugation.
As an example, also with the microstructure unit 107 of multiple array arrangements in micro- channel 101.
As an example, at least one in the surface of the bottom of micro- channel 101, side wall and the microstructure unit 107
Silicon nanowires forest structure is formed on person.
Specifically, the microstructure unit 107 is set on the bottom of micro- channel 101, it is located at micro- channel 101
In the groove profile space of formation, it is preferable that the height of the microstructure unit 107 is identical as the depth of micro- channel 101,
In one preferred embodiment, micro- channel 101 extends in round-trip bending, including several end to end straight line portions and bending
Portion, wherein the microstructure unit 107 can be strip or square block, when being selected as strip, the microstructure unit
107 length is identical as the length of the straight line portion, certainly can be according to other length of actual selection, in addition, the micro-structure list
Member 107 can also be that micro- column structure, the microtrabeculae can be the micro-column structure in round or ellipse section, and size is according to practical
Demand and the selection of micro- channel width.
In addition, in a preferred embodiment, in the bottom 101a and side wall 101b of micro- channel 101, preparing micro-nano
Line forest structure, when being also formed with the microstructure unit 107 in micro- channel 101, also in the microstructure unit
The silicon nanowires forest structure is formed on surface, e.g., when being formed with micro- columnar microstructure unit in micro- channel
When, nano wire forest structure is formed at least one of micro- channel inner wall and the micro-post surface, it is preferable that
The inner wall of micro- channel 101, the surface of the microstructure unit are respectively formed on the nano wire forest structure.Wherein, described
Nano wire forest structure includes multiple silicon nanowires, and it is good that the application is prepared pattern, is evenly distributed, high density and quality is good
Good silicon nanowires forest structure, substantially increases surface area, to effectively improve the column capacity of silicon microfluidic chromatography column, separation
Degree and column effect.Preferably, the line footpath of the silicon nanowires in the silicon nanowires forest structure is between 20~80 nanometers.
In addition, double stationary phase gas chromatographic columns provided by the utility model can be used for Glass Capillary Gas Chromatography Column and
Micro-scale gas chromatograph column based on MEMS.
In order to further illustrate double stationary phase gas chromatographic columns and preparation method thereof of the utility model, provides one and specifically show
Example: it (a) is ready to not yet coat the gas chromatographic column of stationary phase；(b) it prepares stationary phase solution: being prepared by solvent of pentane
The PDMS solution that concentration of volume percent is 4%；It is molten using the PMPS that toluene is 1.7% as solvent dose volume percent concentration
Liquid；(c) at normal temperatures and pressures, configured PDMS solution is injected to color from the port A of gas chromatographic column (first port)
It composes at column suitable position C (predeterminated position), stops injection, seal the port B (second port) of gas chromatographic column；
(d) above-mentioned gas chromatographic column is put into 50 DEG C of vacuum drying oven, after standing 48h, removes B port sealing colloid；So far it completes
The coating of the first stationary phase PDMS, as shown in Figure 2,3；(e) at normal temperatures and pressures, it is injected from the port B of gas chromatographic column
At configured PMPS solution to chromatographic column suitable position C, stop injection, two kinds of stationary phases is made to be connected, seals gas-chromatography
The port A of column；(f) above-mentioned gas chromatographic column is put into 50 DEG C of vacuum drying oven, after standing 48h, removes A port sealing glue
Body；So far the coating for completing second of stationary phase PMPS, as shown in Fig. 4,6.The double stationary phase coating effects of micro-scale gas chromatograph column
Fruit schematic diagram is as shown in figure 4, furthermore, it is noted that in the figure in order to clearly show that double stationary phases coating effects, miniature gas phase color
It composes the upper cover plate of column and is not drawn into.
In conclusion the utility model provides a kind of double stationary phase gas chromatographic columns, double stationary phase gas chromatographic columns include:
Substrate is formed with micro- channel in the substrate, and micro- channel has first port and second port；Encapsulation cover plate, bonding
In the substrate surface, the encapsulation cover plate closes the microchannel that micro- channel forms double stationary phase gas chromatographic columns；
And first stationary phase and the second stationary phase, it is formed in the bottom of micro- channel, side wall and corresponding is located on micro- channel
The inner surface of the encapsulation cover plate of side, and first stationary phase, close to the first port, second stationary phase is close
The second port.Through the above scheme, double stationary phase gas chromatographic columns provided by the utility model and preparation method thereof, same
The coating that two kinds of stationary phases are realized on one gas chromatographic column enables a gas chromatographic column to separate two class gaseous mixtures well
Body component enhances the separating capacity of gas chromatographic column, while reducing to separate and identify variety classes mixing gas component
The frequency of Shi Genghuan gas chromatographic column uses more convenient.So the utility model effectively overcome it is in the prior art
Various shortcoming and have high industrial utilization value.
The above embodiments are only illustrative of the principle and efficacy of the utility model, and not for limitation, this is practical new
Type.Any person skilled in the art can all carry out above-described embodiment under the spirit and scope without prejudice to the utility model
Modifications and changes.Therefore, such as those of ordinary skill in the art without departing from the revealed essence of the utility model
All equivalent modifications or change completed under mind and technical idea, should be covered by the claim of the utility model.
Claims (8)
1. a kind of double stationary phase gas chromatographic columns characterized by comprising
Substrate is formed with micro- channel in the substrate, and micro- channel has first port and second port；
Encapsulation cover plate, is bonded to the substrate surface, and the encapsulation cover plate closes micro- channel and forms double stationary phase gas
The microchannel of phase chromatographic column；And
First stationary phase and the second stationary phase, bottom, side wall and the correspondence for being formed in micro- channel are located on micro- channel
The inner surface of the encapsulation cover plate of side, and first stationary phase, close to the first port, second stationary phase is close
The second port.
2. double stationary phase gas chromatographic columns according to claim 1, which is characterized in that first stationary phase is far from described
The side of first port is in contact with second stationary phase far from the side of the second port.
3. double stationary phase gas chromatographic columns according to claim 1, which is characterized in that first stationary phase includes poly- two
Any one in methylsiloxane layer and polymethylphenylsiloxane layer, second stationary phase includes dimethyl silicone polymer
Layer and polymethylphenylsiloxane layer in any one, first stationary phase is different from second stationary phase.
4. double stationary phase gas chromatographic columns according to claim 1, which is characterized in that micro- channel is in the substrate institute
Plane on the serpentine-like shape of projecting figure, and the edge of the projecting figure be in broken line shape.
5. double stationary phase gas chromatographic columns according to claim 4, which is characterized in that first stationary phase edge is corresponding
The shape of the projecting figure is different from the shape of the corresponding projecting figure in second stationary phase edge.
6. double stationary phase gas chromatographic columns according to claim 1, which is characterized in that the encapsulation cover plate includes two-sided throwing
The encapsulation cover plate is bonded by the glass cover-plate of light using anode linkage method with the substrate.
7. double stationary phase gas chromatographic columns described according to claim 1~any one of 6, which is characterized in that micro- ditch
Also with the microstructure unit of multiple array arrangements in road.
8. double stationary phase gas chromatographic columns according to claim 7, which is characterized in that the bottom of micro- channel, side wall
And silicon nanowires forest structure is formed at least one of surface of the microstructure unit.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110624523A (en) * | 2018-06-22 | 2019-12-31 | 中国科学院上海微系统与信息技术研究所 | Double stationary phase gas chromatographic column and preparation method thereof |
| CN111054185A (en) * | 2020-01-17 | 2020-04-24 | 广东工业大学 | Toxic gas adsorption device and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110624523A (en) * | 2018-06-22 | 2019-12-31 | 中国科学院上海微系统与信息技术研究所 | Double stationary phase gas chromatographic column and preparation method thereof |
| CN110624523B (en) * | 2018-06-22 | 2024-04-02 | 中国科学院上海微系统与信息技术研究所 | Double stationary phase gas chromatographic column and preparation method thereof |
| CN111054185A (en) * | 2020-01-17 | 2020-04-24 | 广东工业大学 | Toxic gas adsorption device and preparation method thereof |
| CN111054185B (en) * | 2020-01-17 | 2024-01-23 | 广东工业大学 | Toxic gas adsorption device and preparation method thereof |
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